Patent GB-755957-A (GB)
Title: Improvements in or relating to the sizing of glass fibers
IPC: C03C25/26
Filed: 1953-10-05
Abstract: Glass fibres are coated with a composition comprising a film-forming saturated polyester resin free from cross linkages and an organo-silicon compound.  Fibres, yarns or fabrics may be treated and coated fibres may be formed into fabrics for subsequent coating with synthetic resinous materials or may be formed into mats, for the production of reinforced plastics.  The polyester component may be obtained by reacting equimolecular proportions of dibasic acids and dihydric alcohols or other polybasic acids and polyhydric alcohols where cross linking can be prevented.  Products mentioned are obtained by reacting succinic acid, oxalic acid, malonic acid, glutaric acid, adipic acid, phthalic acid or the corresponding anhydrides with propylene glycol, ethylene glycol, diethylene glycol, triethylene glycol, butylene glycol, octylene glycol, dipropylene glycol or polyethylene glycol, or a mixture of the acid components with one or more of the glycols, in the presence of triphenyl phosphite at a temperature of 165 DEG  to 200 DEG  C., and in an inert atmosphere formed by bubbling nitrogen or carbon dioxide through the reaction mixture or by reacting the ingredients in solution in toluene or xylene.  At a stage when the product is slightly soluble or dispersible in water, e.g. at an acid number of 25-30 the reaction is stopped by dilution with acetone or by cooling and the product dissolved or dispersed in aqueous ammonium hydroxide to which solution the organo silicon compound is added in aqueous ammonium hydroxide solution.  The organo-silicon compound may be a silane having from 1 to 3 readily hydrolysable groups, e.g. ethoxy, methoxy, chloro, bromo or other halogen groups and an unsaturated organic group having from 2 to 8 carbon atoms or another reactive organic group capable of bonding with the synthetic resinous coating materials.  Examples of the organo compound are sodium vinylpolysiloxanolate and vinyl trichlorosilane.  The size composition may also comprise a polyethylene glycol, dioctylsebacate, di-cocodimethyl ammonium chloride, octadecyl ammonium chloride, tetraethylene pentamine reacted to contain 5 methallyl groups as side chains substituted directly on the nitrogen atoms, pelargonic acid amide, acetic acid, gelatin, polyvinyl acetate or styrene-ester copolymers.  The pH of the size may vary from 4 to 10.  The synthetic resinous materials with which the sized fabrics may be coated or which may be used in the production of reinforced plastics include unsaturated polyesters, polyalkyl acrylates, polystyrene, polyvinylidene chloride, polyvinyl chloride-polyvinyl acetate, phenol formaldehyde or melamine formaldehyde.ALSO:Glass fibres are coated with a composition comprising a film forming saturated poly-ester resin free from cross linkages and an organo-silicon compound. Fibres, yarns or fabrics may be treated and coated fibres may be formed into fabrics for subsequent coating with synthetic resinous materials or may be formed into mats for the production of reinforced plastics.  The polyester component may be obtained by reacting equimolecular proportions of dibasic acids and dihydric alcohols or other polybasic acids and polyhydric alcohols where cross linking can be prevented. Products mentioned are obtained by reacting succinic acid, oxalic acid, malonic acid, glutaric acid, adipic acid, phthalic acid or the corresponding anhydrides with propylene glycol, ethylene glycol, diethylene glycol, triethylene glycol, butylene glycol, octylene glycol, dipropylene glycol or polyethylene glycol, or a mixture of the acid components with one or more of the glycols, in the presence of triphenyl phosphite at a temperature of 165 DEG C. to 200 DEG C., and in an inert atmosphere formed by bubbling nitrogen or carbon dioxide through the reaction mixture or by reacting the ingredients in solution in toluene or xylene.  At a stage when the product is slightly soluble or dispersible in water, e.g. at an acid number of 25-30 the reaction is stopped by dilution with acetone or by cooling and the product dissolved or dispersed in aqueous ammonium hydroxide to which solution the organo silicon compound is added in aqueous ammonium hydroxide solution.  The organo-silicon compound may be a silane having from 1 to 3 readily hydrolysable groups, e.g. ethoxy, methoxy, chloro, bromo or other halogen groups and an unsaturated organic group having from 2 to 8 carbon atoms or another reactive organic group capable of bonding with the synthetic resinous coating materials.  Examples of the organo silicon compound are sodium vinylpolysiloxanolate and vinyl tri-chlorosilane.  The size composition may also comprise a polyethylene glycol, diocetylsebacate, dicocodimethyl ammonium chloride, octadecyl ammonium chloride, tetraethylene pentamine reacted to contain 5 methallyl groups as side chains substituted directly on the nitrogen atoms, pelargonic acid amide, acetic acid gelatine, polyvinyl acetate or styrene-ester copolymers.  The pH of the size may vary from 4 to 10.